Mounting system and sample holder for X-ray diffraction apparatus

ABSTRACT

A mounting system and a sample holder for an X-ray diffraction (XRD) apparatus are provided. The mounting system includes a mounting bracket, an attachment module and a biasing assembly. The mounting bracket is mountable to the XRD apparatus and is rotatable about a rotation axis. The mounting bracket includes an abutment structure defining a reference position. The attachment module is mountable onto the mounting bracket at an adjustable attaching position with respect to the reference position. The attachment module comprises an attaching element that is engageable with the abutment structure for abutting the mounting bracket proximate the reference position. The biasing assembly is mounted onto one of the mounting bracket or the attachment module for interlocking the mounting bracket with the attachment module, such that the mounting bracket is blocked in a plane substantially parallel to the rotation axis, thereby allowing the attaching position to be aligned with the rotation axis.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a Divisional of U.S. application Ser. No. 16/324,256filed on 8 Feb. 2019, now U.S. Pat. No. 10,794,884 B2, which is theNational Stage of International Application No. PCT/CA2017/050947 filedon 10 Aug. 2017, which claims priority to and all advantages of U.S.Provisional Appl. No. 62/372,930 filed on 10 Aug. 2016, the contents ofwhich are hereby incorporated by reference.

FIELD

The technical field generally relates to X-ray apparatus. Moreparticularly, it relates to a mounting system for such apparatus and toa sample holder for holding a sample in the X-ray apparatus.

BACKGROUND

X-ray powder diffraction is a technique commonly used for determiningqualitative and quantitative phase data of a sample, and involvesdirecting an incoming X-ray beam onto a polycrystalline material andrecording the diffracted X-ray beam for analysis. In order to conduct anX-ray diffraction experiment, the sample to be analyzed is generallyplaced on a sample holder which is receivable in part of the X-raydiffractometer. The design of the sample holder is important both forease of use and for obtaining analytical results of good quality. Whilemany types of sample holders are known, existing sample holderstypically exhibit certain shortcomings. For example, reducing backgroundnoise at very low reflection angles (e.g., 0°<θ<3°) is oftenchallenging. Existing sample holders also tend to significantlycontribute to the observed background intensity added to the diffractedpeaks of interest, which may be due to scattering of the X-rays causedby the sample holder material near or directly in contact with thesample. There still exist many challenges in terms of sample holders forX-ray diffractometers.

When assessing structural or mechanical properties of the sample, thesample is typically required to be placed at an appropriate height withrespect to a center of rotation of a goniometer of the instrument, orwith respect with an X-ray source and/or a detector. When a user has towork with multiple attachments or external devices to perform differentkinds of measurements, the position of the sample can be altered fromone attachment or external device to another, as a consequence ofdisparity between the manufacturing and assembly tolerances from onemanufacturer to another. Furthermore, each attachment or external devicetypically has different mechanical fixturing. As a result, adjusting theposition and aligning the sample can be time-consuming. Challenges stillexist in the field of mounting systems for X-ray diffractionapparatuses.

SUMMARY

In some embodiments, a mounting system for an X-ray diffractionapparatus is provided. The mounting system has a rotation axis, andincludes: a mounting bracket rotatably mountable onto the X-raydiffraction apparatus, the mounting bracket being rotatable about therotation axis and including an abutment structure defining a referenceposition with respect to the rotation axis; an attachment moduleadjustably mountable onto the mounting bracket at an attaching position,the attaching position being adjustable along one direction normal tothe reference position, the attachment module including an attachingelement engageable with the abutment structure for abutting the mountingbracket proximate to the reference position; and a biasing assemblymounted onto one of the mounting bracket and the attachment module forinterlocking the mounting bracket with the attachment module, such thatthe mounting bracket is blocked along a plane substantially parallel tothe rotation axis, thereby allowing the attaching position to be alignedwith the rotation axis along said one direction normal to the referenceposition.

In some embodiments, the system includes an adjustment mount operativelyconnected to the attachment module for adjusting the attaching positionof the attachment module.

In some embodiments, the adjustment mount has a bottom portion andcomprises a micrometer screw mechanically connected with said bottomportion.

In some embodiments, the abutment structure includes: a first abutmentelement having a vertically-extending portion; and a second abutmentelement having a horizontally-extending portion.

In some embodiments, the attaching element is matably engageable with atleast one of the first and second abutment elements.

In some embodiments, the first abutment element includes a notch and theattaching element includes a recess engageable with the notch.

In some embodiments, the notch is dove-tailed.

In some embodiments, the notch includes a machined inner portion.

In some embodiments, the attaching element includes a snap-lockmechanism cooperating with the mounting bracket.

In some embodiments, the system includes a sample holder mounted ontothe attachment module.

In some embodiments, the system includes a non-ambient stage mountedonto the attachment module.

In some embodiments, the biasing mechanism is a lever rotatably mountedonto the mounting bracket.

In some embodiments, the rotation axis passes through a center ofrotation of a goniometer.

In some embodiments, a method for mounting a mounting system onto anX-ray diffraction apparatus is provided. The method includes steps ofdefining a mounting position; providing a mounting bracket proximate themounting position; rotatably mounting the mounting bracket to the X-raydiffraction apparatus; and affixing the mounting bracket to the X-raydiffraction apparatus.

In some embodiments, the method includes a step of defining a referenceposition.

In some embodiments, the method includes a step of determining aposition of a rotation axis of a goniometer.

In some embodiments, the step of affixing the mounting bracket to theX-ray diffraction apparatus includes mechanically rigidly connecting themounting bracket with the X-ray diffraction apparatus.

In some embodiments, the method includes steps of providing anattachment module engageable with the mounting bracket; engaging theattachment module with the mounting bracket; interlocking the attachmentmodule and the mounting bracket; and adjusting an attaching position ofthe attachment module with respect with the reference position.

In some embodiments, a method for aligning an attachment module with amounting bracket having an abutment structure and being mounted onto anX-ray diffraction apparatus is provided. The method includes steps ofmounting a first attachment module having an attaching element onto themounting bracket; abutting the attaching element to the abutmentstructure proximate a reference position; interlocking the firstattachment module to the mounting bracket; and adjusting an attachingposition of the first attachment module with respect with the referenceposition.

In some embodiments, the interlocking step includes engaging a biasingmechanism with the attaching element or the mounting bracket.

In some embodiments, the method includes steps of unlocking the firstattachment module from the mounting bracket; detaching the firstattachment module from the mounting bracket; replacing the firstattachment module onto the mounting bracket; interlocking the firstattachment module to the mounting bracket; and verifying the attachingposition of the first attachment module.

In some embodiments, the method includes steps of detaching the firstattachment module from the mounting bracket; mounting a secondattachment module onto the mounting bracket; abutting the secondattachment module to the abutment structure proximate the referenceposition; interlocking the second attachment module to the mountingbracket; and adjusting an attaching position of the first attachmentmodule with respect with the reference position.

In some embodiments, the interlocking the second attachment module tothe mounting bracket step includes engaging a biasing mechanism with theat least one attaching element or the mounting bracket.

In some embodiments, the method includes steps of unlocking the secondattachment module from the mounting bracket; detaching the secondattachment module from the mounting bracket; replacing the secondattachment module onto the mounting bracket; interlocking the secondattachment module to the mounting bracket; and verifying the attachingposition of the second attachment module.

In some embodiments, there is provided a sample holder and a method ofcarrying out X-ray diffraction measurements on a sample to be analyzed.

In some embodiments, a sample holder for an X-ray diffraction apparatusis provided. The sample holder includes: an insert including an uppersurface and a sample space for holding a sample; and an insert housing,including: a first surface having an outer edge and an inner edge; asecond surface opposite to the first surface; a sidewall connecting thefirst surface to the second surface and forming an opening therebetween, the opening being adapted to removably receive the inserttherein; and a retention assembly for retaining the insert in theopening, the retention assembly including: flange members provided onthe first surface and extending above the opening; and a biasingassembly for biasing at least part of the upper surface of the insertagainst the flange members such that the upper surface of the insert isflush with the first surface, the flange members being positioned withrespect to one another so as to define an unobstructed channel extendingfrom a first portion of the outer edge to a second opposed portion ofthe outer edge.

In some embodiments, the sample space includes a depression defined inthe upper surface of the insert.

In some embodiments, the depression has a depth between about 2 mm and10 mm.

In some embodiments, the sample space is located substantially at thecenter of the insert.

In some embodiments, the insert housing has an annular shape and theinsert has a cylindrical shape.

In some embodiments, the flange members and the upper surface areengaged along at least 50% of the perimeter of the upper surface of theinsert, or at three or more widely spaced points of the perimeter of theupper surface of the insert.

In some embodiments, the flange members have a thickness of at leastabout 1 mm.

In some embodiments, the insert housing is made of metal. In someembodiments, the insert housing is made of plastic, ceramic or a singlecrystal semiconductor.

In some embodiments, the metal includes at least one of steel, brass andaluminum.

In some embodiments, the channel is defined along a projection path ofan incoming X-ray beam from the X-ray diffraction apparatus and areflection X-ray beam reflected off the sample.

In some embodiments, the flange members are positioned with respect toone another so as to define a second channel extending from a thirdportion of the outer edge to a fourth portion of the outer edge andthrough the sample space, such that the upper surface of the insert isflush with the first surface along the second channel.

In some embodiments, an anti-scatter baffle is receivable along thesecond channel. In some embodiments, an anti-scatter baffle is mountableon top of the flange members, and runs along the length or diameter ofthe sample holder and of the sample space, above the sample space.

In some embodiments, the anti-scatter baffle is positionable above theupper surface of the insert, for example at a height lower than a heightof the second channel.

In some embodiments, an insert housing of a sample holder for an X-raydiffraction apparatus is provided. The insert housing includes: a firstsurface having an outer edge and an inner edge; a second surfaceopposite to the first surface; a sidewall connecting the first surfaceto the second surface and forming an opening there between, the openingbeing adapted to removably receive an insert therein, the insertincluding an upper surface and a sample space for holding a sample; anda retention assembly for retaining the insert in the opening, theretention assembly including: flange members provided on the firstsurface and extending above the opening, the flange members beingpositioned so as to define a channel extending from a first portion ofthe outer edge of the first surface to a second opposed portion of theouter edge of the first surface and through the sample space; and abiasing assembly for biasing at least part of the upper surface of theinsert against the flange members such that the upper surface of theinsert is flush with the first surface at least along the channel.

In some embodiments, an insert is provided which is insertable in asample holder of an X-ray diffraction apparatus, and includes: an uppersurface made of amorphous PVC; and a sample space defined in the uppersurface, for holding a sample. In some embodiments, the amorphouspolymer is amorphous PVC.

In some embodiments, the insert is made of an amorphous material. Inother embodiments, the insert is made of ceramic, a semiconductormaterial, a metal or a polymer. In some embodiments, the insert is madeof a crystalline (polycrystalline or single crystalline) material havingan X-ray diffraction signal which does not interfere with the X-raydiffraction signal of the sample to be analyzed. In some embodiments,the insert is made of a single crystalline material which is oriented toavoid background diffraction peaks in directions of interest for thesample.

In some embodiments, an insert insertable in a sample holder of an X-raydiffraction apparatus is provided. The insert includes: an uppersurface; a sample space defined in the upper surface, for holding asample; and a standard reference space defined in the upper surface, forholding a standard reference substance.

In some embodiments, a sample holder for an X-ray diffraction apparatusis provided. The sample holder comprises: an insert comprising an uppersurface and a sample space for holding a sample; and an insert housing,comprising: a sidewall defining an opening, the sidewall having a topsurface having an outer edge and an inner edge, and a bottom surfaceopposite the top surface, the opening being adapted to removably receivethe insert therein; and a retention assembly for retaining the insert inthe opening, the retention assembly comprising: flange members providedon the top surface and extending above the opening; and a biasingassembly for biasing at least part of the upper surface of the insertagainst the flange members such that the upper surface of the insert isflush with the top surface, the flange members being positioned withrespect to one another so as to define an unobstructed channel extendingfrom a first portion of the outer edge to a second opposed portion ofthe outer edge.

In some embodiments, the sample space comprises a depression defined inthe upper surface of the insert.

In some embodiments, the depression has a depth between about 2 mm and10 mm.

In some embodiments, the sample space is located substantially at thecenter of the insert.

In some embodiments, the upper surface of the insert has a substantiallyannular shape.

In some embodiments, the sample space has a substantially circularshape.

In some embodiments, the insert housing has a substantially annularshape and the insert has a substantially cylindrical shape.

In some embodiments, the flange members and the upper surface areengaged along at least 50% of the perimeter of the upper surface of theinsert.

In some embodiments, the flange members have a thickness of at leastabout 1 mm.

In some embodiments, the flange members are substantially flat.

In some embodiments, the flange members have a plate construction.

In some embodiments, the flange members have a substantially annularsector shape.

In some embodiments, the flange members have outer and inner curvededges and side edges, each side edge being substantially parallel withrespect to a side edge of an adjacent flange member to define part ofthe channel.

In some embodiments, each of the flange members comprises an overhangportion configured for abutting against the upper surface of the insert.

In some embodiments, the insert housing is made of metal.

In some embodiments, the metal comprises at least one of steel, brassand aluminum.

In some embodiments, the channel is defined along a projection path ofan incoming X-ray beam from the X-ray diffraction apparatus and areflection X-ray beam reflected off the sample.

In some embodiments, the flange members are positioned with respect toone another so as to define a second channel extending from a thirdportion of the outer edge to a fourth portion of the outer edge andthrough the sample space, such that the upper surface of the insert isflush with the top surface along the second channel.

In some embodiments, the second channel is configured to receive ananti-scatter baffle therealong.

In some embodiments, the anti-scatter baffle is positionable above theupper surface of the insert at a height lower than a depth of the secondchannel.

In some embodiments, there is provided an insert housing of a sampleholder for an X-ray diffraction apparatus. The insert housing comprises:a sidewall defining an opening, the sidewall having a top surface havingan outer edge and an inner edge, and a bottom surface opposite the topsurface, the opening being adapted to removably receive an inserttherein, the insert comprising an upper surface and a sample space forholding a sample; and a retention assembly for retaining the insert inthe opening, the retention assembly comprising: flange members providedon the top surface and extending above the opening, the flange membersbeing positioned so as to define a channel extending from a firstportion of the outer edge of the top surface to a second opposed portionof the outer edge of the top surface and through the sample space; and abiasing assembly for biasing at least part of the upper surface of theinsert against the flange members such that the upper surface of theinsert is flush with the top surface at least along the channel.

In some embodiments, the insert housing has a substantially annularshape.

In some embodiments, the flange members and the upper surface areengagable along at least 50% of the perimeter of the upper surface ofthe insert.

In some embodiments, the flange members have a thickness of at leastabout 1 mm.

In some embodiments, the flange members are substantially flat.

In some embodiments, the flange members have a plate construction.

In some embodiments, the flange members have a substantially annularsector shape.

In some embodiments, the flange members have outer and inner curvededges and side edges, each side edge being substantially parallel withrespect to a side edge of an adjacent flange member to define part ofthe channel.

In some embodiments, each of the flange members comprises an overhangportion configured for abutting against the upper surface of the insert.

In some embodiments, the insert housing is made of metal.

In some embodiments, the metal comprises at least one of steel, brassand aluminum.

In some embodiments, the flange members are positioned with respect toone another so as to define a second channel extending from a thirdportion of the outer edge to a fourth portion of the outer edge andthrough the sample space, such that the upper surface of the insert isflush with the top surface along the second channel.

In some embodiments, the second channel is configured to receive ananti-scatter baffle therealong.

In some embodiments, the anti-scatter baffle is positionable above theupper surface of the insert at a height lower than a depth of the secondchannel.

In some embodiments, an insert insertable in a sample holder of an X-raydiffraction apparatus is provided. The insert comprises: an uppersurface made of amorphous PVC; and a sample space defined in the uppersurface, for holding a sample.

In some embodiments, an insert insertable in a sample holder of an X-raydiffraction apparatus is provided. The insert comprises: an uppersurface; a sample space defined in the upper surface, for holding asample; and a standard reference space defined in the upper surface, forholding a standard reference substance.

In some embodiments, the standard reference space is a protuberancewhich is flush with the upper surface and in which the standardreference substance is embedded.

Other features will be better understood upon reading of embodimentsthereof with reference to the appended drawings.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a top perspective view of a mounting system, according to anembodiment.

FIG. 2 is a front view of the mounting system of FIG. 1.

FIG. 3 is a top perspective view of an attachment module held inproximity to a mounting system, according to an embodiment.

FIG. 4 is a top perspective view of the attachment module of FIG. 3about to be engaged with the mounting system of FIG. 3.

FIG. 5 is a top perspective view of the attachment module of FIG. 3engaged with the mounting system of FIG. 3.

FIG. 6 is a top perspective view of an attachment module interlockedwith a mounting system, according to an embodiment.

FIG. 7 is a top view the attachment module interlocked with the mountingsystem of FIG. 6.

FIG. 8 is a top perspective view of a mounting system interlocked withan attachment module mounted onto a sample holder, according to anembodiment.

FIG. 9 is a top perspective view of a mounting system interlocked withan attachment module mounted onto a non-ambient stage, according to anembodiment.

FIG. 10 is a workflow chart illustrating an example of a method formounting a mounting system to an X-ray diffraction apparatus and foraligning an attachment module with a mounting bracket mounted onto theX-ray diffraction apparatus, according to an embodiment.

FIG. 11 is a top perspective view of a sample holder including an inserthousing and an insert, according to an embodiment.

FIG. 12 is a top perspective view of the insert housing of the sampleholder of FIG. 11.

FIG. 13 is a partial top perspective cross-sectional view of the sampleholder of FIG. 11.

FIG. 14 is a partial top perspective view of the insert housing of FIG.12.

FIG. 15 is a bottom perspective view of the insert housing of FIG. 12.

FIG. 16a is an exploded view of the sample holder of FIG. 11.

FIG. 16b is a further exploded view of the sample holder of FIG. 16 a.

FIG. 17 is a top perspective view of a sample holder including an inserthousing and an insert having a deep depression, according to anotherembodiment.

FIG. 18 is a top perspective view of the sample holder of FIG. 11,provided with an anti-scatter baffle.

FIG. 19 is a top perspective view of the sample holder of FIG. 11,mounted on an X-ray diffractometer (X-ray diffractometer partiallyshow).

FIG. 20 is a top plan view of the sample holder of FIG. 11, showing theconfiguration of the flange members.

FIG. 21 is a top plan view of a sample holder including two flangemembers, according to another embodiment.

FIG. 22 is a top plan view of a sample holder including multiple flangemembers, according to yet another embodiment.

FIG. 23 is a top plan view of a sample holder including two flangemembers, according to yet another embodiment.

FIG. 24 is a partial top plan view of an insert having a sample spaceand a standard reference space, according to yet another embodiment.

FIG. 25 is a partial top plan view of an insert having a sample spaceand a standard reference space, according to yet another embodiment.

FIG. 26 is a partial top plan view of an insert having a sample spaceand a circular standard reference space, according to yet anotherembodiment.

DETAILED DESCRIPTION

In the following description, similar features in the drawings have beengiven similar reference numerals. In order to not unduly encumber thefigures, some elements may not be indicated on some figures if they werealready mentioned in preceding figures. It should also be understoodherein that the elements of the drawings are not necessarily drawn toscale and that the emphasis is instead being placed upon clearlyillustrating the elements and structures of the present embodiments.

The present description generally relates to a mounting system for anX-ray diffraction apparatus, which will be referred to as a “universalmounting system”, as it could be mounted on any kind (i.e. type and/orbrand) of X-ray diffraction apparatus.

Moreover, it will be appreciated that positional descriptions such as“top”, “bottom”, “under”, “left”, “right”, “front”, “rear”, “adjacent”,“opposite”, “parallel”, “perpendicular”, “inner”, “outer”, “internal”,“external”, and the like should, unless otherwise indicated, be taken inthe context of the figures and should not be considered limiting.

In the present disclosure, the following terminology and expressions mayalso be used:

The terms “X-ray”, “X-radiation”, “light”, “electromagnetic radiation”,“optical”, “spectral profile” “spectral waveband”, derivatives andvariants thereof, are used to refer to radiation in any appropriateregion of the electromagnetic spectrum and, more particularly, are notlimited to visible light. By way of example, the X-rays may cover orsubstantially correspond to wavelengths ranging from 0.01 to 10nanometers (i.e. frequencies in the range of 30 petahertz to 30exahertz), which may be of particular interest for applications in thematerials science industry for investigating the structural (e.g. atomicstructure) or mechanical (e.g. residual stress) properties of samples.

The terms “sample”, “sample under investigation”, “material”, “analyzedsample”, “powder”, “thin films”, derivatives and variants thereof areused to refer to a quantity of matter extracted or taken apart from alarger amount for analysis, or may refer to matter that is eithernatural (e.g. a specific chemical element found in nature), synthesized(e.g. a reaction of chemical compounds), or man-made (e.g. a powerformed by scratching a thin film). It will be understood that the sampleintrinsically has various physical and chemical properties, which may beassessed using different instruments and methods (e.g. XRD analysis).

The terms “diffractometer”, “X-ray diffraction apparatus”, “XRDdiffraction system”, “powder diffraction instruments”, “X-rayapparatus”, derivatives and variants thereof refer to an apparatusconfigured to acquire patterns obtained by recording the intensities ofX-rays scattered by the sample under investigation at different anglesbetween an incident beam (i.e. beam incident on the sample) and ascattered beam (also referred to as “reflected beam”). The acquiredpatterns are typically representative of given properties (e.g.structure) of the material to be inspected. The above-mentionedapparatus could further be understood as a device configured to senseand/or probe x-rays scattered and/or reflected by the surface to beinspected, according to the needs of a particular application. It willbe understood that different attachments (also referred to as “externaldevice”, e.g. different kinds of sample holders or the like) may beattached to the XRD apparatus.

Mounting System and Method

The mounting system and related elements and/or components that will bedescribed herein are particularly useful in the field of materialsanalysis. Although such system and related elements and/or componentsmay be particularly useful for allowing high-precision positioning ofattachment for X-ray apparatus, they may also be aimed at otherapplications, such as different kinds of microscope or other opticalassembly or system in which positioning of a sample at a precise,reliable and repeatable location may be needed.

As previously mentioned, some embodiments may be useful in the field ofX-ray powder diffraction when, for example, the atomic and/or molecularstructure of a crystal has to be identified, or when residual stress ofmaterials has to be assessed. Embodiments of the mounting system andassociated XRD apparatus are described below as they have been designedfor use in the field of material inspection, but they may of course beused in the broad field of non-destructive inspection, testing orevaluation, in which XRD analysis only serves the purpose of a usefulexample.

As one skilled in the art would readily understand, some of the X-raydiffraction apparatuses typically (but not necessarily) include agoniometer allowing an object (e.g. a detector and/or a source) to berotated to a precise angular position with respect to a center ofrotation. A rotation axis may pass through the center of rotation, and,as such, defines an axis about which an X-ray source and/or a detectormay rotate. The rotation axis may then be referred to as “the rotationaxis of the goniometer” or, alternatively, “the rotation axis of the XRDapparatus”. In the following, the rotation axis will be understood asbeing an axis comprised in a plane extending substantially parallel toan “XY plane” and crossing the center of rotation. In the currentdescription, the “XY plane” is defined as a plane substantially parallelto (or a plane coinciding with) a surface of the sample to becharacterized. Conversely, the surface of the sample lies in a planesubstantially parallel to the XY plane or in a plane coinciding with theXY plane. In such scenario, a “Z direction” or, alternatively, a “Zaxis”, and variants thereof (e.g. “Z plane”) will hence be understood asthe axis being substantially perpendicular to the XY plane (i.e. thesurface of the sample). Broadly, the present description will refer tothe “X, Y, Z planes” as being three perpendicularly intersecting planes,but as it will be readily understood, the angle between the planes mayvary (e.g. the angle formed at the intersection of the X and Y planesmay be different than 90 degrees, or the angle formed at theintersection of the Z plane with the XY plane may be different than 90degrees). For the sake of clarity and concision of the presentdescription, the XY plane will herein be referred to as lying in ahorizontal plane (i.e. a horizontal direction), while the Z axis will bereferred to as lying in a vertical plane (i.e. a vertical direction).

The XRD apparatus may include, in addition to the goniometer, an X-raysource (including, for example, a vacuum-sealed X-ray tube), an X-raygenerator delivering high tension current to the X-ray source, a sampleholder to hold the sample to be investigated, an X-ray detector capableof detecting X-ray and/or X-ray photons scattered by the sample and anX-ray optical assembly (typically used for collimating, conditioning, orfocusing the X-rays at the detector).

As it has been previously mentioned, the XRD pattern is obtained byrecording the intensities of X-rays scattered by the sample at differentangles between the beam incident on the sample and beam scattered by thesample. When it is required to use different attachments (hereinreferred to as “external devices”) for assessing the properties of thesample, it is hence crucial, for obtaining significant and reliableresults, that the sample is maintained at the same position with respectto the X-ray source and X-ray detector from one attachment to another.

Referring to FIGS. 1 and 2, a mounting system 20 for an X-raydiffraction apparatus is shown. In some implementations, the XRDapparatus may include a shaft mounted onto the X-ray diffractionapparatus near or at the center of rotation of the goniometer.

The mounting system 20 includes a mounting bracket 22. The mountingbracket 22 is rotatably mountable onto the X-ray diffraction apparatus,for example near the center of rotation of the goniometer. In someimplementations, the mounting bracket 22 is rotatably mounted onto theshaft of the XRD apparatus, and is aligned with both the shaft of theX-ray diffraction apparatus and the center of rotation of thegoniometer), as it will be described with greater details below. It willbe understood that the term “aligned” generally refers to an arrangementin appropriate relative positions between the mounting bracket 22 andthe XRD apparatus (or any other elements or group(s) of elements). Forexample, a central portion of the mounting bracket 22 may be alignedwith a portion the XRD apparatus, or the rotation axis of the goniometer(i.e. the rotation axis may pass through the central portion of themounting bracket 22).

As illustrated, the mounting bracket 22 has a substantially circularouter edge 23 and has a central hole 25. The mounting bracket 22 may bemade from any solid material such as stainless steel, brass, aluminum,copper. Of course, the mounting bracket 22 could have variousgeometrical configurations (i.e. size and dimensions), and could, forexample, have a triangular, rectangular, circular, or any other shapedbody and/or outer edge 23, as dictated by one's needs. The size of themounting bracket 22 is typically influenced by the dimensions of theexternal device to be mounted onto the mounted bracket.

The central hole 25 may have a circular shape so as to allow an affixingmeans to be inserted therein. The affixing means could be, but are notlimited to bolts, screws, or any other elements allowing the mountingbracket 22 to be affixed to the X-ray diffraction apparatus, when thecentral hole 23 or a portion of the central hole is aligned with therotations axis of the XRD apparatus. Different geometricalconfigurations are also possible. For example, the mounting bracketcould include a plurality of holes for allowing a plurality of affixingmeans to be inserted therein, so as to be affixed the mounting bracket22 to the XRD apparatus, as already known by one skilled in the art.

Different components and/or means may be used to mount the mountingbracket 22 onto the XRD apparatus. For example, a snap-lock mechanismmay be provided onto the XRD apparatus and the mounting bracket, so asthe mounting bracket is properly aligned with respect with the rotationaxis of the goniometer. Alternatively, various affixing means,including, but not limited to glue, screws, clips, welding, magnets,variants and combinations thereof could be used. As it will be readilyunderstood, the mounting bracket 22 substantially remains at the sameposition (i.e. horizontal and vertical positions) as the one it has beenmounted (i.e. the alignment has to be maintained) while being freelyrotatable about the rotation axis of the XRD apparatus, and variousmechanical means and components to achieve this objective could be used.In some implementations, the mounting bracket 22 may be rotatable aboutthe shaft of the XRD apparatus.

Still referring to FIGS. 1 and 2, the mounting bracket 22 also includesan abutment structure 24 defining a reference position 26. The referenceposition 26 is in spatial relationship with the central hole 25, and sois also in spatial relationship with the rotation axis of thegoniometer. The reference position 26 defines a position, or moreparticularly, a relative height (herein defined as being normal to theXY plane, or the surface of the sample) to which may be mounted theexternal device(s), as it will be described with greater details later.In the illustrated variant, the reference position 26 is located belowthe central hole 25. In the following, the reference position 26 isdefined by a transverse axis of the mounting bracket 22. The transverseaxis lies in the XY plane.

As illustrated in FIGS. 1 and 2, the abutment structure 24 includes afirst abutment element 24A having a vertically-extending portion and asecond abutment element 24B having a horizontally-extending portion,meaning that the first and second abutment elements 24A,24B aresubstantially perpendicular (the first lies in the Z plane, while thesecond lies in the XY plane). Alternatively, the first and secondabutment elements 24A,24B could be disposed at an angle different than90 degrees with respect to each other, or may even be parallel to eachother. In the later configuration (i.e. the two elements 24A, 24B beingparallel), the first abutment element 24A may be provided near a topportion of the mounting bracket 22, while the second abutment element24B may be provided near a bottom portion of the mounting bracket 22 (orvice-versa). Alternatively, the first abutment element 24A may beprovided near a left portion of the mounting bracket 22, while thesecond abutment element 24B may be provided near a right portion of themounting bracket 22 (or vice-versa). In such configurations, the twoelements 24A,24B are spaced apart from the central hole 25.

The first and second abutment elements 24A, 24B are mounted andmechanically affixed to the mounting bracket 22, but may optionally beformed directly in/from the mounting bracket 22. In this configuration,the mounting bracket 22 forms an integrated piece (i.e. a monolithicelement) having two protuberances extending outwardly from a surface ofthe mounting bracket 22. Alternatively, at least one of the first andsecond abutment elements 24A, 24B could be a notch, a recess or acombination thereof. It will be understood that he first and secondabutment elements 24A,24B encompass a large variety of components andmeans allowing an external device to be mounted to the mounting bracket22.

In some embodiments, the first and/or second abutment elements 24A,24Bmay have an inner portion. Optionally, the inner portion may be profiledand/or machined. For example, the inner portion of the first and/orsecond abutment elements 24A,24B could have a notch or a groove (alsoreferred to as a “slide”) defining a dovetail profile, so as to beengageable with a compatible piece having a corresponding dovetailprofile (i.e. the dovetail profile of the first and/or second abutmentelements 24A,24B is the “negative image” of the dovetail profile of thecompatible piece). The inner portion may further be machined ormicromachined to provide a texture, a slope, a geometrical configurationor any other properties to the inner portion, according to one's needs.

At least one of the first and second abutment elements 24A, 24B could bereplaced by various components or structures. For example, they could bereplaced by holes to allow appropriate positioning of the externaldevice onto the mounting bracket 22. By way of an example, the first andsecond abutment elements 24A, 24B may comprise a snap-lock mechanismcooperating with the external device.

As it has been previously mentioned, the external device may be a sampleholder, a non-ambient stage, or any other elements need for a targetedapplication.

Now referring to FIGS. 3 to 9, the mounting system 20 also includes anattachment module 28 mountable onto the mounting bracket 22 at anadjustable attaching position 30 with respect to the reference position26, the attaching position 30 extending in a Z direction 38. Asillustrated, the Z direction 38 is substantially perpendicular to the XYplane (i.e. the surface of the sample). As it has been alreadymentioned, the Z direction 38 will be understood as a “verticaldirection”, and the expression “attaching position 30 of the attachmentmodule 28 in” has to be understood as the adjustable attaching position30 of the attachment module 28. More particularly, the attachingposition 30 may be adjusted so as the attachment module 28 is “aligned”,i.e. at a proper height with respect with the reference position 26,and/or with respect with the X-ray source and detector. In someimplementations, the attaching position 30 is adjustable along onedirection normal to the reference position 26, and so the attachingposition 30 may be aligned with the rotation axis along the directionnormal to the reference position 26.

The attachment module 28 is typically provided on the external device 41and includes at least one attaching element 34 (also referred to as “theattaching element 34”). The attaching element 34 is engageable with theabutment structure 24 for abutting the mounting bracket proximate thereference position 26, and hence allow to position the external device41 with respect to the reference position 26.

In the illustrated variant, the attaching element 34 is mechanicallyconnected to the external device 41 via a support plate 29 affixed tothe attaching element 34 at one end and to the external device 41 atanother end. Consequently, when the attaching position 30 is adjusted,the attaching element 34 and/or the external device 41 may be translated(i.e. may be adjusted) along the Z direction 38.

The attaching element 34 may be provided with a notch or a groove (alsoreferred to as a “slide”) to enable a repeatable placement of theexternal device. Similarly to the first and second abutment elements24A, 24B, the attaching element 34 is mechanically designed to allowrepeated positioning with high precision (order of magnitude of theprecision in the microns).

More particularly, the attaching element 34 is designed, sized and hasthe geometrical configuration so as to be mountable onto any kinds ofexternal device (e.g. sample holder or non-ambient stage) and compatiblewith the mounting bracket 22 (i.e. with the abutment structure 24).Consequently, the design and the geometrical features of the attachingelement 34 are similar to the ones of the abutment structure 24, or moreprecisely, the first and second abutment elements 24A,24B (i.e. they mayabut and may be considered as compatible and/or engageable). Optionally,the attaching element 34 may be matably engageable with a correspondingat least one of the first and second abutment elements 24A, 24B.

When the attaching element 34 is mounted to the mounting bracket 22 viathe abutment structure 24, the attaching element 34 is blocked in the XYdirections, and only an adjustment in the Z direction 38 may berequired. This feature can be advantageous, for example, when one has touse different external devices, as it may substantially diminish theamount of time required to perform the adjustment. Indeed, the externaldevice 41 has to be adjusted according to only one axis (herein referredto as a Z axis extending in the Z direction), instead of three axes (X,Y and Z). It is to be mentioned that one may need to pre-align theattachment module 28, the attaching element 34 and/or the externaldevice 41 the first time the mounting system 20 is used. Thepre-alignment may include an adjustment along one, two or threedirections (defined by the X, Y, and/or Z axis).

The mounting system 20 further includes an adjustment mount 40 foradjusting the attaching position 30 of the attachment module 28 alongthe Z direction 38. The adjustment mount 40 may be mounted directly onthe attaching element 34 or may be mounted onto the external device 41,as long as the adjustment mount 40 allows translating the attachmentmodule 28 onto which is mounted the external device 41. Optionally, theattaching element 34 and/or the external device 41 may translate alongthe Z direction 38. For example, the external device 41 may be affixedto the attaching element 34, and the attaching element 34 may betranslatable along the Z direction 38 (i.e. the attaching element 34 mayslide in the mounting bracket 22, thereby translating the externaldevice 41, or vice versa).

In some embodiments, the adjustment mount 40 has a bottom portion 42 andcomprises a screw 44 mechanically connected with the bottom portion. Thescrew 44 may be a micrometer screw or a differential screw.Alternatively, the screw 44 may be replaced by any other component(s) ormechanism allowing to make small and precise adjustment to the attachingposition 30.

The mounting system 20 also includes a biasing assembly 36 mounted ontoone of the mounting bracket 22 or to the attachment module 28 forinterlocking the mounting bracket 22 with the attachment module 28, suchthat the mounting bracket 22 is blocked along the XY plane (i.e. themounting bracket may not move in the XY plane or the horizontaldirection). For example, the biasing assembly 36 could be mounted oneither the sides or the top portions of one of the mounting bracket 22or the attachment module 28. As it has been previously mentioned, theexternal device 41 hence only needs to be adjusted along one verticaldirection (e.g. the Z direction 38).

The mechanism 36 may include levers with screw and/or threaded hole(s),locking knob, spring plungers, combinations thereof, or any othermechanical component allowing to interlock the mounting bracket 22 withthe attaching element 34.

As illustrated, the biasing assembly 36 is a lever rotatably mountedonto the mounting bracket 22 and is free to rotate about its head. Thelever may be rotated from an unlock angular position 37 to a lockangular position 39. When the lever is in the unlock angular position37, the attaching element 34 may be put in contact (i.e. engaged) withthe abutment structure 24 (through the first and second abutmentelements 24A, 24B). Conversely, the attaching element 34 may also bedisengaged from the abutment structure 24. In use, the attaching element34 abuts the abutment structure 24, and the lever in is the lock angularposition: 39 the attaching element 34 is thus blocked in the XY plane.

Some embodiments of a mounting assembly are illustrated in FIGS. 8 and9. The mounting assembly is typically similar to the mounting system,but further comprises an external device 41 mechanically connected tothe attaching element 34. The external device 41 may be, for example, asample holder (FIG. 8) or a non-ambient stage (FIG. 9). In bothexamples, the external device 41 is interlocked with the mountingbracket 22. The attaching position 30 of the attachment module 28 mayonly be adjusted along the Z direction 38 (i.e. the attachment module 28may not move in the X and Y directions).

In some scenarios, the mounting system 20 and assembly disclosed in thepresent description can provide an easy-to-install and easy-to-alignmounting bracket 22, as compared to existing mounting systems andbracket.

In some embodiments, the mounting bracket 22 is equipped with aminiature slide (i.e. a “groove” or a “notch”) that may have, forexample, a dovetail profile. The mounting bracket 22 can be engageablewith an attachment module 28 including at least one attaching element34, so as to enable a repeatable placement of external devices. Themounting bracket 22 also allows positioning the external devices withhigh precision (order of magnitude of the precision in the microns).Furthermore, the mounting system 20 can be configured to be “universal”,meaning that it could be mounted onto an existing XRD apparatus (i.e.XRD apparatus known in the art).

In some scenarios, the angle between the sample and the incident beam ismodified during the measurements. This can typically be achieved inseveral ways, for example: (i) fixed source, rotating sample, movingdetector (θ/2θ mode); (ii) fixed sample, moving source, moving detector(θ/θ mode); or (iii) fixed detector, moving source, rotating sample(2θ/θ mode). It is to be noted that the mounting system described aboveis compatible with the different aforementioned detection modes (i.e.θ/2θ, θ/θ and/or 2θ/θ).

It is also to be noted that the mounting system described above may beconfigured to be mountable onto either bench scale XRD apparatus or fulllaboratory XRD system. It is understood that the differentcharacteristics of the XRD apparatus such as the size, the power, theresolution and/or the like should not limit the use of the mountingsystem presented in the current description.

In accordance with embodiments, there is also provided a method formounting a mounting system onto an X-ray diffraction apparatus having arotation axis. The method includes steps of: defining a mountingposition, providing a mounting bracket proximate the mounting position,rotatably mounting the mounting bracket to the X-ray diffractionapparatus, and affixing the mounting bracket to the X-ray diffractionapparatus.

In some embodiments, the method includes a step of defining a referenceposition.

In some embodiments, the method includes a step of determining aposition of a rotation axis of a goniometer.

In some embodiments, the step of aligning the portion of the mountingbracket with the center of rotation includes defining a referenceposition in spatial relationship with the center of rotation.

In some embodiments, the step of affixing the mounting bracket to theX-ray diffraction apparatus comprises mechanically rigidly connectingthe mounting bracket with the X-ray diffraction apparatus.

In some embodiments, the method for mounting a mounting system onto anX-ray diffraction may further comprise steps of: providing an attachmentmodule engageable with the mounting bracket, engaging the attachmentmodule with the mounting bracket, interlocking the attachment module andthe mounting bracket, and adjusting an attaching position of theattachment module with respect with the reference position.

For example, the method may include steps of mechanically connecting theattachment module with an external device and adjusting a horizontalposition of the external device. As it has been previously stated, thehorizontal position is in spatial relationship with the center ofrotation.

In accordance with embodiments, there is also provided a method foraligning an attachment module with a mounting bracket having an abutmentstructure and being mounted onto an X-ray diffraction apparatus.

The method may include step of mounting a first attachment module havingan attaching element onto the mounting bracket, abutting the attachingelement to the abutment structure proximate a reference position,interlocking the first attachment module to the mounting bracket, andadjusting an attaching position of the first attachment module withrespect with the reference position.

In some embodiments, the interlocking step comprises engaging a biasingmechanism with the attaching element or the mounting bracket.

In some embodiments, the method may include at least some of thefollowing steps: unlocking the first attachment module from the mountingbracket, detaching the first attachment module from the mountingbracket, replacing the first attachment module onto the mountingbracket, interlocking the first attachment module to the mountingbracket, verifying the attaching position of the first attachment moduleand detaching the first attachment module from the mounting bracket.

In some embodiments, the method may include at least some of thefollowing steps, mounting a second attachment module onto the mountingbracket, abutting the second attachment module to the abutment structureproximate the reference position, interlocking the second attachmentmodule to the mounting bracket, and adjusting an attaching position ofthe first attachment module with respect with the reference position.

In some embodiments, the step of interlocking the second attachmentmodule to the mounting bracket comprises engaging a biasing mechanismwith the at least one attaching element or the mounting bracket

In some embodiments, the method may further comprise at least some ofthe following steps: unlocking the second attachment module from themounting bracket, detaching the second attachment module from themounting bracket, replacing the second attachment module onto themounting bracket, interlocking the second attachment module to themounting bracket, and verifying the attaching position of the secondattachment module.

In some embodiments, the interlocking step includes engaging a biasingmechanism with the at least one attaching element or the mountingbracket.

The method may comprise additional steps aimed at verifying thealignment between the first attachment module and the center of rotation(i.e. confirming that the alignment is appropriate, and maintained fromone measurement to another). Such additional steps may include, forexample a step of unlocking the first attachment module from themounting bracket, a step of detaching the first attachment module fromthe mounting bracket, a step of replacing the first attachment moduleonto the mounting bracket, a step of interlocking the first attachmentmodule to the mounting bracket and a step of verifying the alignmentbetween the first attachment module and the center of rotation of thegoniometer.

When a user needs to change from one external device (connected to afirst attachment module) to another (connected to a second attachmentmodule), the method may include a step of detaching the first attachmentmodule from the mounting bracket, a step of mounting a second attachmentmodule having at least one attaching element onto the mounting bracket,a step of interlocking the second attachment to the mounting bracket anda step of adjusting the horizontal position of the second attachmentmodule.

FIG. 10 illustrates an example of a workflow chart representing a methodthat may be used for mounting the mounting system to the XRD apparatusand/or aligning an attachment module with a mounting bracket having anabutment structure and being mounted onto an X-ray diffractionapparatus. This example combines some of the embodiments which has beenpreviously introduced, but may also comprise additional steps to ensurea proper alignment of the mounting bracket, the attachment module, theattaching element and/or the external device, as it will be readilyunderstood by one skilled in the art.

In some embodiments, a method for pre-aligning each external device maycomprise the steps of placing and replacing the external device.

The step of placing the external device may comprise sub-steps of:mounting the external device, locking the external device in place witha lever, aligning the external device to the center of rotation usingthe attaching element, unlocking the lever, and removing the externaldevice.

The step of replacing the external device may include sub-steps of:replacing the external device and checking the alignment again. Thesesteps may be followed by sub-steps of: removing the external device,mounting a second external device 41′, locking the second externaldevice in place, aligning the second external device 41 to the center ofrotation using the attaching element, unlocking the lever, removing thesecond external device, replacing the second external device, andchecking the alignment again.

For a subsequent use, the user may just mount any external device, lockit in place and verify the alignment along the Z axis.

The method as presented in the current description can allow for ahigh-precision positioning of external devices. Furthermore, in somescenarios, the time associated with the alignment can be reduced or evensignificantly reduced, as the alignment is performed in only onedirection (the Z axis). The user only has to replace (i.e. change) theexternal device and may quickly perform measurements, after a briefverification of the alignment.

It is appreciated that features of one of the above describedembodiments can be combined with the other embodiments, variants oralternatives thereof.

Moreover, although the embodiments of the mounting bracket, abutmentstructure, attachment module, attaching element, biasing assembly andcorresponding parts thereof consist of certain geometricalconfigurations as explained and illustrated herein, not all of thesecomponents and geometries are essential and thus should not be taken intheir restrictive sense. It is to be understood, as also apparent to aperson skilled in the art, that other suitable components andcooperation thereinbetween, as well as other suitable geometricalconfigurations (dimensions, shape, and the like), may be used for themounting bracket, abutment structure, attachment module, attachingelement and biasing Full

Sample Holder

The following section provides embodiments of a sample holder for anX-ray diffraction apparatus, which may be used for conductingmeasurements at very low reflection angles (e.g., 0°<6<3°), whilemaintaining a low background noise. The sample holder includes an insertfor holding the sample, and an insert housing into which the insert isreceivable.

Referring to FIGS. 11 to 16, a sample holder 100 for an X-raydiffractometer is shown. The sample holder 100 includes an inserthousing 104 and an insert 102 receivable in the insert housing 104. Theinsert housing 104 includes a first surface (or top surface) 108 and asecond surface (or bottom surface) 110 opposite to the first surface108. The first surface 108 and the second surface 110 are connected by asidewall 112, thereby defining an opening 114 between the first surface108 (at a first end of the sidewall 112) and the second surface 110 (ata second end of the sidewall 112). In some embodiments, the inserthousing can be made of metal, which can be at least one of steel andaluminum. In some embodiments, the insert 102 can be made of a polymermaterial, as will be described in further detail below.

In the embodiment shown on FIGS. 11 to 16, the first surface 108 is anannulus having a circular outer edge 108 a and a circular inner edge 108b. The second surface 110 has a generally annular shape provided withrecesses 120, and the opening 114 is a through-hole defined between thefirst surface 108 and the second surface 110, such that the inserthousing 104 is ring-shaped. It is understood that in other embodiments,the size and shape of the first surface 108, the second surface 110 andthe sidewall 112 can vary, depending on the X-ray diffractometer used.For example, the insert housing 104 can have a rectangular shape or anyother suitable shape. It is also understood that the opening 114 is notnecessarily a through-hole. For example, the opening 114 can be open atthe first end of the sidewall 112, and closed at the second end of thesidewall 112. In some embodiments, the second surface 110 can bedirectly used as a supporting surface for setting the sample holder 100onto a measurement platform of the X-ray diffractometer, as shown onFIG. 19.

In some embodiments, the opening 114 is adapted to receive the insert102. It is understood that by “adapted to receive the insert”, it ismeant that the opening 114 is sized such that the insert 102 can fittherein. In the embodiment shown on FIGS. 11 to 16, the insert 102 isinsertable into the insert housing 104 from the second end of theopening 114. However, it is understood that other configurations can beused for introducing the insert 102 into the opening 114. For example,in alternate embodiments, the insert housing can be made of at least twoseparate parts configured to be joined together and secured around theinsert.

Still referring to FIGS. 11 to 16, in some embodiments, the inserthousing 104 is configured to securely retain the insert 102 in positionso as to allow for the X-ray diffraction measurement to be performed(i.e., for retaining the insert in a substantially immobile positionwhile the X-ray diffraction measurement is performed). In order toretain the insert 102 in position, the insert housing 104 is providedwith a retention assembly for retaining the insert 102 in the opening114. In some embodiments, all or part of the retention assembly can besupported by the first surface 108. Embodiments of the retentionassembly will be discussed in further detail below.

Now referring to FIGS. 11, 13 and 16, in some embodiments, the insert102 has an upper surface 116 and a sample space 106 onto which a sample(not shown) is positionable for exposure to an X-ray beam. In someembodiments, the upper surface 116 can completely surround the samplespace 106, and the sample space 106 can be located in a substantiallycentral area of the upper surface 116. In some embodiments, the samplespace 106 includes a depression defined in the upper surface 116. It isunderstood that the size, shape and location of the depression may vary,depending on the configuration of the insert housing, and on the nature,form and quantity of sample to be analyzed. For example, when the sampleto be analyzed is a powder, the user can select a sample space 106(i.e., select an insert 102 having a certain sample space 106) having asmall depth (e.g., between 0.2 mm and 1 mm) and fill the sample space106 with the powder such that the top of the powder deposit issubstantially flush with the upper surface 116.

Alternatively, and now referring to FIG. 17, when the sample to beanalyzed has a larger dimension (e.g., a metallic piece or a chunk ofmineral), the user can select a sample space 106 having a greater depth(e.g., up to 10 mm). The greater depth can allow for directly submittinglarge samples to X-ray diffraction analyses without the need to scrapeoff small amounts of material from the sample, or otherwise damage thesample.

Now referring to FIGS. 11 to 16 and 20, the retention assembly caninclude flange members 117 against which the insert 102 can be abutted,and a biasing assembly for biasing the insert against the flange members117. In the embodiment shown, the flange members 117 are arranged alonga circumference of the insert housing 104. Each one of the flangemembers 117 includes a first portion 117 a provided on the first surface108, and a second portion 117 b (i.e., an overhang portion) extendingfrom the inner edge 108 b of the first surface 108 to above the opening114. In order to retain the insert 102 in a substantially immobileposition in the opening 114, part of the upper surface 116 of the insert102 can be abutted against the flange members 117, for example against abottom surface 117 c of the second portion 117 b of the flange members117. The flange members 117 can have a thickness 117 d which is chosendepending on the material used and the length of the flange members,such that the insert 102 is securely held in position. In someembodiments, the flange members 117 can be made of the same material asthe insert housing so long as the material is suitable for securelyholding the insert 102 in position.

It is understood that the size, shape and location of the flange members117 can vary. It is also understood that the thickness 117 d, the lengthof the first portion 117 a, the length of the second portion 117 b andthe area of the bottom surface 117 c can vary. For example, the firstportion 117 a can span from the outer edge 108 a of the first surface108 to the inner edge 108 b of the first surface 108, as seen in FIGS.11 to 16 and 20. In alternate embodiments, for example as shown on FIGS.21 and 23, the first portion 117 a does not span the entire width of thefirst surface 108.

In some embodiments, the retention assembly includes a biasing assemblyfor biasing the insert 102 against the flange members 117 (e.g. againstthe bottom surface 117 c of the flange members 117). In the embodimentshown on FIGS. 11 to 16, the biasing assembly includes a groove 118provided between the second surface 110 and an inner portion 119 of thesidewall 112, recesses 120 provided in the second surface 110, and abiasing clip 122 having two opposed ends 122 a, 122 b. The biasing clip122 is removably engageable with the groove 118 by inserting each of theopposed ends 122 a, 122 b in one of the corresponding recesses 120. Thegroove 118 is sized and shaped such that rotating the biasing clip 122about axis A while the biasing clip 122 is engaged in the groove 118biases the insert 102 against the flange members 117. In the embodimentshown, the biasing clip 122 is rotated 90° in order to bias the insert102 against flange members 117, but it is understood that the inserthousing can be configured so that other rotation angles may be used. Itis also understood that other types of biasing assemblies may be used tobias the insert 102 against flange members 117. For example, the biasingassembly can include a spring or a plurality of springs for biasing theinsert 102 against flange members 117.

In some embodiments, the flange members 117 are positioned with respectto one another so as to define at least one channel. Each of the atleast one channel extends from a first portion of the outer edge locatedon one side of the sample space 106 to a second portion of the outeredge which is located on an opposite of the sample space 106. Thebiasing assembly biases at least part of the upper surface 116 of theinsert 102 against the flange members 117 such that the upper surface116 is flush with the first surface. This provides an unobstructed pathalong each of the at least one channel, which can allow an X-ray beam tobe directed towards and reflected off the sample at low reflectionangles, such as angles between 0° and 3°. It should be understood thatthe term “flush”, when used to describe the positioning of two surfaceswith respect to one another, means that the two surfaces aresubstantially leveled, for example with a margin of error of about ±10micron.

In the embodiment shown on FIGS. 11 to 16 and 20, four flange members117 are provided on the first surface 108. Each flange member 117 isshaped as an annular sector. The first portion 117 a of each flangemember 117 spans across the first surface 108, from the outer edge 108 ato the inner edge 108 b, and the second portion 117 b extends from thefirst portion 117 a to above the opening 114. In the embodiment shown,the flange members 117 have a thickness of about 0.5 mm, and areelevated with respect to the first surface 108. As can be seen on FIG.20, the flange members 117 are spaced apart on the first surface 108 soas to define a first channel 124 and a second channel 126 orthogonal tothe first channel 124. The first channel 124 extends from a firstportion 128 of the outer edge 108 to a second portion 128′ of the outeredge 108 opposite to the first portion 128. Similarly, the secondchannel 126 extends from a first portion 130 of the outer edge 108 to asecond portion 130′ of the outer edge 108. When the insert 102 is biasedagainst the flange members 117, the upper surface 116 of the insert isflush with the first surface 108, which creates an unobstructed pathalong each one of the channels 124, 126. It is understood that in otherembodiments, the second channel is not necessarily orthogonal to thefirst channel.

Now referring to the embodiment shown on FIG. 21, two flange members 117are provided on the first surface 108. Each flange member 117 is shapedas an annular sector. The first portion 117 a of the flange members 117extends from inner edge 108 b and covers a portion of the first surface108, but does not reach the outer edge 108 a. The second portion 117 bextends from the first portion 117 a to above the opening 114. Theflange members 117 are spaced apart on the first surface 108 so as todefine a channel 124. The channel 124 extends from a first portion 128of the outer edge 108 to a second portion 128′ of the outer edge 108opposite to the first portion 128. When the insert 102 is biased againstthe flange members 117, the upper surface 116 of the insert is flushwith the first surface 108, which creates an unobstructed path along thechannel 124.

Now referring to the embodiment shown on FIG. 22, four flange members117 are provided on the first surface 108 to define the channel 124 asdiscussed above, and two secondary flange members 134 are provided onthe first surface 108. In some scenarios, the secondary flange members134 can provide additional stability to the insert 102.

Now referring to the embodiment shown on FIG. 23, two flange members 117are provided on the first surface 108. In this embodiment, the portionof the first surface 108 which is not covered by the flange members 117is larger than the portion of the first surface 108 which is covered bythe flange members 117. The flange members 117 are positioned withrespect to one another such that the width of the unobstructed pathdefined by the channel 124 is wider when closer to an outer edge 108 aof the first surface 108.

Referring to FIGS. 20 to 23, the channel 124 is defined along aprojection path of an X-ray beam emitted from the X-ray diffractionapparatus and reflected off a sample placed in the sample space 106. Asthe channel 124 is unobstructed, the incident and reflection angles ofthe X-ray beam can be lowered (for example lowered to between 0° and 3°)without being blocked or hindered by the flange members. Thisconfiguration can allow performing low-angle X-ray diffraction analyseswhile reducing background noise and keeping the sample in a suitableposition (i.e., substantially immobile with respect to the inserthousing) to be analyzed.

Now referring to the embodiment shown on FIGS. 18 and 20, the secondchannel 126 enables an anti-scatter baffle 132 to be positioned to aheight which is lower than the thickness of the flange members 117. Theanti-scatter baffle 132, also referred to as an anti-scatter “knifeedge” or “blade”, may be useful for limiting or blocking diffractedX-ray from all but the directions associated with the sample beingtested, thereby helping to improve the signal-to-noise ratio of thedetected signal. As it can be advantageous to position the anti-scatterbaffle 132 as close as possible to the sample, this configuration canallow further improving the signal-to-noise ratio. In some embodiments,the anti-scatter baffle 132 is attached to the frame of the X-raydiffractometer and can be lowered down close to the sample space. Theanti-scatter baffle 132 can be made of any material which is dense (orheavy) and does not fluoresce, such as tungsten.

In some embodiments, the flange members 117 and the first surface 108form an integral structure (i.e., the flange members 117 and the firstsurface 108 can be a one-piece structure). In other embodiments, theflange members 117 and the first surface 108 are separate pieces and theflange members 117 can be affixed to the first surface 108 using afastener. For example, the flange members 117 can be bolted or screwedonto the first surface 108.

In order to fulfill the focusing conditions required to conduct an X-raydiffraction measurement at different diffraction angles, the anglebetween the sample and the incident beam is typically modified duringthe course of the measurement. This can typically be achieved in severalways, such as

-   -   (i) fixed source, rotating sample, moving detector (θ/2θ mode);    -   (ii) fixed sample, moving source, moving detector (θ/θmode); or    -   (iii) fixed detector, moving source, rotating sample (2θ/θ        mode).

For conducting a measurement in the θ/θ mode using the sample holder ofthe present description, it is understood that the sample holder can bekept in a fixed position (so that the sample placed in the sample spaceis in a fixed position) and that the X-ray source can be aligned suchthat the path of the incoming X-ray beam and the path of the reflectedX-ray beam passes above the channel. In other words, such that theprojection of the incoming X-ray beam and the projection of thereflected X-ray beam is in the plan defined by the first surface 108 ofthe insert housing 104 and the upper surface 116 of the insert 102. Withthis configuration, measurements at low diffraction angles (such asbetween 0° and 3°) can be performed, as the X-ray beams are notobstructed by the flange members 117.

For conducting a measurement in the 2θ/θ mode or θ/2θ mode, it isunderstood that the sample holder can be rotated about axis A (so thatthe sample placed in the sample space rotates). In such case,measurements at low diffraction angles (such as between 0° and 3°) canbe performed for certain rotation angles, for example when theprojection path of the incoming and reflected X-ray beams isunobstructed (i.e., is in the plan defined by the first surface 108 ofthe insert housing 104 and the upper surface 116 of the insert 102). Formeasurements in the 2θ/θ mode or θ/2θ mode, the thickness of the flangemembers can be chosen to be as small as possible while being thickenough to securely retain the insert, so as to allow limiting theobstruction of the incoming and reflected X-ray beams by the flangemembers 117.

In some embodiments and as described herein, the insert 102 can be madeof a plastic material. In some embodiments, the upper surface 116 of theinsert 102 can be made of a polymer selected from the group consistingof amorphous PVC. In some embodiments, the insert 102 is a one-piecestructure made of such an amorphous polymer. It has been found thatusing amorphous PVC can lower the scattering of the X-ray, which can inturn reduce background noise.

In order to identify a substance using powder X-ray diffraction,comparison of the diffraction pattern of a sample with the diffractionpattern of a known standard reference compound can be performed. TheX-ray diffraction pattern of the standard reference is typicallyrecorded separately from the sample to identify (i.e., prior to or afterrecording the X-ray diffraction pattern of the sample to identify). Thiscan require dismounting the sample holder from the X-ray diffractionapparatus, taking the insert out of the insert housing and cleaning orreplacing the insert prior to performing a second separate measurement.It has been found that the insert 102 can be configured so as to reducethe number of measurements performed, for example by recording the X-raydiffraction pattern of the sample and the standard reference substanceat the same time. Possible configurations are discussed in furtherdetail with reference to FIGS. 24 and 25 below.

Now referring to FIGS. 24 to 26, in some embodiments, a sample space 106for holding a sample to be analyzed and a standard reference space 140for holding a reference substance can both be defined in the uppersurface 116 of the insert 102. It is understood that the sample space106 and the reference space 140 are separate spaces defined in the uppersurface 116 and can both be simultaneously or consecutively exposed tothe X-ray beam when the X-ray diffraction apparatus is operated. In somescenarios, the standard reference space 140 can be embodied by a spacewhich can removably receive a standard reference substance therein. Inother scenarios, the standard reference space 140 can be embodied by aprotuberance which has a top surface flush with the upper surface of theinsert, and which has a standard reference substance embedded therein.For example, the protuberance can be made of the same material as theinsert and have the standard reference substance embedded therein.

In the embodiment shown on FIG. 24, the circular sample space 106 isdivided into a first semi-circular sample space 106 a and a secondsemi-circular sample space 106 b. The sample to be analyzed can beplaced in the semi-circular sample spaces 106 a and 106 b. In someembodiments, the standard reference space 140 can be a rectangular stripprovided between the semi-circular sample spaces 106 a and 106 b. Insuch case, a standard reference substance can be placed in the standardreference space 140, such that the top of the standard referencesubstance is leveled with the top of the sample placed in the samplespaces 106 a, 1065 b. In other embodiments, the standard reference space140 can be a rectangular protuberance which contains the standardreference substance. For example, the rectangular protuberance can bemade of the same material as the insert and the standard referencesubstance can be embedded within the standard reference space. In suchcase, the rectangular protuberance is configured such that its topsurface is flush with the upper surface of the insert. The X-raydiffraction pattern of both the sample and the standard referencesubstance can be recorded simultaneously.

In the embodiment shown on FIG. 25, the standard reference space 140 ispositioned such that the circular sample space 106 is divided into twouneven circle segments 106 a (minor segment) and 106 b (major segment).In the embodiment shown on FIGS. 16a and 16b , the standard referencespace 140 is an annulus provided around the sample space 106. It isunderstood that the size, shape and relative positioning of the standardreference space 140 and the sample space 106 can vary.

It is appreciated that features of one of the above describedembodiments can be combined with the other embodiments or alternativethereof.

Moreover, although the embodiments of the sample holder, insert housing,insert and corresponding parts thereof consist of certain geometricalconfigurations as explained and illustrated herein, not all of thesecomponents and geometries are essential and thus should not be taken intheir restrictive sense. It is to be understood, as also apparent to aperson skilled in the art, that other suitable components andcooperation thereinbetween, as well as other suitable geometricalconfigurations, may be used for the sample holder, insert housing, andinsert of the present description.

It will further be understood that the mounting sample and the sampleholder presented in the current description could either be use on theirown or in combination. More particularly, the sample holder could bemounted to the mounting system so as to obtain a “universal sampleassembly”. Such configurations may be practical in the context ofperforming reliable measurements, for example measurements requiringboth a high-precision positioning of attachment(s) for X-ray apparatusand/or for conducting measurements at very low reflection angles. Theabove described embodiments of the mounting system may hence be combinedwith embodiments of the sample holder.

Several alternative embodiments and examples have been described andillustrated herein. The embodiments described above are intended to beexemplary only. A person skilled in the art would appreciate thefeatures of the individual embodiments, and the possible combinationsand variations of the components. A person skilled in the art wouldfurther appreciate that any of the embodiments could be provided in anycombination with the other embodiments disclosed herein. The presentexamples and embodiments, therefore, are to be considered in allrespects as illustrative and not restrictive. Accordingly, whilespecific embodiments have been illustrated and described, numerousmodifications come to mind without significantly departing from thescope defined in the appended claims.

The invention claimed is:
 1. A method for mounting a mounting systemonto an X-ray diffraction apparatus, the method comprising: defining amounting position; providing a mounting bracket proximate the mountingposition; rotatably mounting the mounting bracket to the X-raydiffraction apparatus; affixing the mounting bracket to the X-raydiffraction apparatus; providing an attachment module engageable withthe mounting bracket; engaging the attachment module with the mountingbracket; interlocking the attachment module and the mounting bracket;defining a reference position; and adjusting an attaching position ofthe attachment module with respect with the reference position.
 2. Themethod of claim 1, wherein the step of affixing the mounting bracket tothe X-ray diffraction apparatus comprises mechanically rigidlyconnecting the mounting bracket with the X-ray diffraction apparatus. 3.A method for aligning an attachment module with a mounting brackethaving an abutment structure and being mounted onto an X-ray diffractionapparatus, the method comprising steps of: mounting a first attachmentmodule having an attaching element onto the mounting bracket; abuttingthe attaching element to the abutment structure proximate a referenceposition; interlocking the first attachment module to the mountingbracket; and adjusting an attaching position of the first attachmentmodule with respect with the reference position.
 4. The method of claim3, wherein the interlocking step comprises engaging a biasing mechanismwith the attaching element or the mounting bracket.
 5. The method ofclaim 3, further comprising steps of: unlocking the first attachmentmodule from the mounting bracket; detaching the first attachment modulefrom the mounting bracket; replacing the first attachment module ontothe mounting bracket; interlocking the first attachment module to themounting bracket; and verifying the attaching position of the firstattachment module.
 6. The method of claim 5, further comprising stepsof: detaching the first attachment module from the mounting bracket;mounting a second attachment module onto the mounting bracket; abuttingthe second attachment module to the abutment structure proximate thereference position; interlocking the second attachment module to themounting bracket; and adjusting an attaching position of the firstattachment module with respect with the reference position.
 7. Themethod of claim 6, wherein the interlocking the second attachment moduleto the mounting bracket step comprises engaging a biasing mechanism withthe at least one attaching element or the mounting bracket.
 8. Themethod of claim 7, further comprising steps of: unlocking the secondattachment module from the mounting bracket; detaching the secondattachment module from the mounting bracket; replacing the secondattachment module onto the mounting bracket; interlocking the secondattachment module to the mounting bracket; and verifying the attachingposition of the second attachment module.